CN116409839A - NMP waste liquid purification system and technology - Google Patents
NMP waste liquid purification system and technology Download PDFInfo
- Publication number
- CN116409839A CN116409839A CN202310688422.1A CN202310688422A CN116409839A CN 116409839 A CN116409839 A CN 116409839A CN 202310688422 A CN202310688422 A CN 202310688422A CN 116409839 A CN116409839 A CN 116409839A
- Authority
- CN
- China
- Prior art keywords
- nmp
- heating kettle
- waste liquid
- molecular sieve
- sieve membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 70
- 239000002699 waste material Substances 0.000 title claims abstract description 54
- 238000000746 purification Methods 0.000 title claims abstract description 21
- 238000005516 engineering process Methods 0.000 title abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 66
- 239000002808 molecular sieve Substances 0.000 claims abstract description 50
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000012528 membrane Substances 0.000 claims abstract description 49
- 238000004821 distillation Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002351 wastewater Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims description 17
- 239000012535 impurity Substances 0.000 claims description 11
- 239000012530 fluid Substances 0.000 claims description 4
- 239000006258 conductive agent Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000003204 osmotic effect Effects 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 56
- 238000005265 energy consumption Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 238000005373 pervaporation Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- QGKLPGKXAVVPOJ-UHFFFAOYSA-N pyrrolidin-3-one Chemical compound O=C1CCNC1 QGKLPGKXAVVPOJ-UHFFFAOYSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007581 slurry coating method Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/043—Details
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/10—Energy recovery
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application relates to an NMP waste liquid purification system and technology, which belong to the technical field of matched equipment for lithium ion battery production. The system comprises: heating kettle, distillation tower, roots blower, buffer tank, molecular sieve membrane group, condenser, wastewater receiving tank, product receiving tank, vacuum buffer tank and vacuum pump; the heating kettle is used for heating NMP waste liquid to be purified, the bottom of the heating kettle is provided with a gas distributor, and the gas outlet end at the top of the heating kettle is respectively connected with a distillation tower and a molecular sieve membrane group; the air inlet end of the gas distributor is connected with a Roots blower; and the molecular sieve membrane group is used for separating NMP and water molecules in the circulating treatment gas. According to the process provided by the invention, through regulating and controlling the osmotic pressure and the air pressure of the Roots blower, the NMP waste liquid is circularly dehydrated in a gas phase form, so that NMP purification is realized.
Description
Technical Field
The invention relates to the technical field of waste resource utilization, in particular to an NMP waste liquid purification system and technology.
Background
NMP (N-methyl pyrrolidone) is a slurry mixed solvent used in the production of new energy batteries such as lithium ion batteries, sodium ion batteries and the like. NMP waste liquid recovered after slurry coating can be reused after being purified to be qualified. The existing NMP waste liquid purification technology mainly adopts rectification, but the rectification process needs to convey part of condensed fraction back into the tower for reheating, so the energy consumption is higher. Besides rectification, pervaporation has also been used for purifying NMP waste liquid, and the principle is that NMP waste liquid is conveyed into an assembly having a molecular sieve membrane or an organic polymer membrane suitable for passing water molecules but not suitable for passing NMP molecules to separate NMP and water, and the technology faces the problems that impurities such as metal ions, organic polymers and the like in the waste liquid are in direct contact with a permeable membrane, and can adhere to the membrane assembly or ion exchange with metal ions on the membrane, so that the service life of the membrane is affected, and when the NMP concentration in the waste liquid is high, NMP in the waste liquid also permeates through the permeable membrane, so that the NMP content of the permeable waste water is high, and the treatment cost of the permeable waste water is increased.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an NMP waste liquid purification system and a NMP waste liquid purification process. The NMP waste liquid is gasified, so that moisture is separated from impurities, and the moisture is removed through a molecular sieve, so that the aim of NMP purification is fulfilled.
The invention provides an NMP waste liquid purification system, which comprises: heating kettle, distillation tower, roots blower, buffer tank, molecular sieve membrane group, condenser, wastewater receiving tank, product receiving tank, vacuum buffer tank and vacuum pump;
the heating kettle is used for heating NMP waste liquid to be purified, the bottom of the heating kettle is provided with a gas distributor, and the gas outlet end at the top of the heating kettle is respectively connected with a distillation tower and a molecular sieve membrane group; the air inlet end of the gas distributor is connected with a Roots blower;
the distillation tower is used for separating the NMP waste liquid with qualified moisture, the air inlet end at the bottom of the distillation tower is connected with the air outlet end of the heating kettle, and the air outlet end at the top of the distillation tower is connected with the condenser;
the molecular sieve membrane group is used for separating NMP and water molecules in the circulating treatment gas; the inlet of the heating kettle is connected with the air outlet end of the heating kettle; the outlet of the upper end is connected with a condenser and discharges water molecules, and the outlet of the lower end is connected with a buffer tank and discharges NMP circulation treatment gas after removing a part of water molecules;
the Roots blower is used for circularly treating the air to be pressurized and then blown into the bottom of the heating kettle; the air inlet end of the air inlet pipe is connected with a buffer tank;
the condenser is used for condensing the distilled material steam, and the air inlet end of the condenser is connected with the air outlet end of the distillation tower and the upper end outlet of the molecular sieve membrane group; the air outlet end of the device is connected with a waste water receiving tank and a product receiving tank;
the vacuum buffer tank is used for reducing the pressure of the system, the inlet end of the vacuum buffer tank is respectively connected with the wastewater receiving tank and the product receiving tank, and the outlet end of the vacuum buffer tank is connected with the vacuum pump;
the vacuum pump is used for reducing pressure of the system and exhausting tail gas, and the inlet end of the vacuum pump is connected with the outlet end of the vacuum buffer tank.
Further, the wastewater receiving tank and the product receiving tank are used for collecting wastewater and NMP products, respectively.
Further, a valve is arranged between the heating kettle and the distillation tower.
Further, a valve is arranged between the heating kettle and the molecular sieve membrane group.
Further, the molecular sieve in the molecular sieve membrane group is NaA molecular sieve, and the aperture is 4A.
A purification process for NMP waste liquid using the above system, comprising:
adding NMP waste liquid to be purified into a heating kettle, removing non-condensable gas under the pressure of less than or equal to-0.099 MPa, closing a valve on the heating kettle, and heating to 120+/-5 ℃ until the temperature of the waste liquid is 120 ℃; when the Roots blower is started and the Roots blower blows air into the kettle liquid, the circulating treatment gas forms small bubbles which are uniformly distributed through the gas distributor, carries out heat and mass exchange with the kettle liquid, and water molecules enter the bubbles and then enter the gas phase of the liquid surface, and finally enter the molecular sieve membrane group to separate NMP and water molecules; at this time, the condenser is filled with a refrigerating fluid at the temperature of-15 to-10 ℃ and the absolute pressure of the permeation side of the molecular sieve membrane group is controlled to be less than 2kPa;
when the water content of NMP waste liquid circulated into the heating kettle is less than or equal to 100ppm, a valve of the heating kettle, which is communicated with a distillation tower, is opened, a valve communicated with a molecular sieve membrane group is closed, cooling water with the temperature less than or equal to 32 ℃ is introduced into a condenser, absolute pressure in the heating kettle is controlled to be 7-10kPa, kettle liquid temperature is controlled to be 128-134 ℃, distillation tower top temperature is controlled to be 118+/-1 ℃, and NMP in the kettle liquid is distilled out, so that impurity ions, polymers and conductive agent impurities are removed.
Further, the wind pressure of the Roots blower outlet is 10000h+ (1000-2000) Pa, wherein h is the liquid level height (unit is m) in the heating kettle.
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. compared with rectification, the invention has no reflux and lower energy consumption than rectification; the Roots blower pressurizes and does work on the circulating gas to increase the temperature of the circulating gas, and the heat can be used for heating waste liquid to reduce the energy consumption of system operation.
2. Compared with pervaporation, the NMP waste liquid in the invention does not directly contact the molecular sieve membrane component, so that unless the air pressure of the Roots blower exceeds a set value due to misoperation, organic polymers and metal ions in the waste liquid cannot contact the molecular sieve membrane, and the service life of the molecular sieve membrane component can be prolonged.
3. Because the volatility of water is far greater than that of NMP, when the water content of NMP waste liquid is less than or equal to 100ppm, the concentration ratio of water molecules and NMP molecules in the gas phase is also greater than that in the liquid phase, so that compared with pervaporation, the NMP content in the permeable waste water passing through the molecular sieve is lower.
4. According to the invention, the kettle bottom gas distributor is designed in the heating kettle, so that the gas entering the kettle is uniformly distributed, and the winding efficiency of the equipment is improved.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the NMP waste liquid purification system of the present invention;
FIG. 2 is a cross-sectional view of a heating kettle in the NMP waste liquid purification system of the present invention;
FIG. 3 is a top view of a gas distributor in a heating kettle of the NMP waste liquid purification system of the present invention.
Reference numerals:
1. heating the kettle; 2. a molecular sieve membrane group; 3. a buffer tank; 4. roots blower; 5. a distillation column; 6. a condenser; 7. a wastewater receiving tank; 8. a product receiving tank; 9. a vacuum buffer tank; 10. a vacuum pump; 11. a gas distributor.
Detailed Description
In order to make the above objects, features and advantages of the present application more comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. This application is, however, susceptible of embodiment in many other forms than those described herein and similar modifications can be made by those skilled in the art without departing from the spirit of the application, and therefore the application is not to be limited to the specific embodiments disclosed below.
In this application, unless specifically stated and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art as the case may be.
An NMP waste liquid purification system, as shown in fig. 1-3, comprising: a heating kettle 1, a molecular sieve membrane group 2, a buffer tank 3, a Roots blower 4, a distillation tower 5, a condenser 6, a wastewater receiving tank 7, a product receiving tank 8, a vacuum buffer tank 9 and a vacuum pump 10;
the heating kettle 1 is used for heating NMP waste liquid to be purified, the bottom of the heating kettle is provided with a gas distributor 11, the gas inlet end of the gas distributor 11 is connected with a Roots blower 4, and the gas outlet end at the top of the heating kettle is respectively connected with a distillation tower 5 and a molecular sieve membrane group 2;
the distillation tower 5 is used for separating NMP waste liquid with qualified water, the air inlet end at the bottom of the distillation tower is connected with the air outlet end of the heating kettle 1, and the air outlet end at the top of the distillation tower is connected with the condenser 6;
a molecular sieve membrane group 2 for separating NMP and water molecules in the circulating treatment gas; the inlet of the heating kettle is connected with the air outlet end of the heating kettle 1; the outlet at the upper end of the device is connected with a condenser 6 and discharges water molecules, the outlet at the lower end of the device is connected with a buffer tank 3 and NMP circulation treatment gas after removing the water molecules is discharged;
the Roots blower 4 is used for circularly treating the bottom of the heating kettle 1 after pressurizing; the air inlet end of the air inlet pipe is connected with a buffer tank 3;
the condenser 6 is used for condensing the distilled material steam, and the air inlet end of the condenser is connected with the air outlet end of the distillation tower 5 and the upper end outlet of the molecular sieve membrane group 2; the air outlet end is connected with a waste water receiving tank 7 and a product receiving tank 8;
the vacuum buffer tank 9 is used for reducing the pressure of the system, the inlet end of the vacuum buffer tank is respectively connected with the wastewater receiving tank 7 and the product receiving tank 8, and the outlet end of the vacuum buffer tank is connected with the vacuum pump 10;
the vacuum pump 10 is used for system depressurization and exhaust, and the inlet end of the vacuum pump 10 is connected with the outlet end of the vacuum buffer tank 9.
In a preferred embodiment, a wastewater receiving tank 7 and a product receiving tank 8 are used to collect wastewater and NMP product, respectively.
In a preferred embodiment, a valve is provided between the heating vessel 1 and the distillation column 5.
In a preferred embodiment, a valve is arranged between the heating kettle 1 and the molecular sieve membrane group 2.
In a preferred embodiment, the molecular sieve in the molecular sieve membrane group 2 is a NaA molecular sieve, and the pore size is 4A.
A purification process for NMP waste liquid using the above system, comprising:
adding NMP waste liquid to be purified into a heating kettle 1, removing non-condensable gas under the pressure of less than or equal to-0.099 MPa, closing a valve on the heating kettle 1, which is communicated with a distillation tower 5, and heating to the temperature of the waste liquid of 120+/-5 ℃; when the Roots blower 4 is started, the Roots blower 4 blows air into the kettle liquid, the circulating treatment gas forms uniformly distributed small bubbles through the gas distributor 11, carries out heat and mass exchange with the kettle liquid, and water molecules enter the bubbles and then enter the gas phase of the liquid surface, and finally enter the molecular sieve membrane group 2 to separate NMP and water molecules; at this time, the condenser 6 is filled with a refrigerating fluid at the temperature of-15 to-10 ℃ and the absolute pressure of the permeation side of the molecular sieve membrane group 2 is controlled to be less than 2kPa;
when the water content of NMP waste liquid circulated into the heating kettle 1 is less than or equal to 100ppm, opening a valve of the heating kettle 1 which is communicated with the distillation tower 5, closing a valve which is communicated with the molecular sieve membrane group 2, changing a condenser 6 into cooling water with the temperature less than or equal to 32 ℃, controlling the absolute pressure in the heating kettle 1 to be 7-10kPa, the kettle temperature to be 128-134 ℃ and the distillation tower top temperature to be 118+/-1 ℃, and distilling NMP in the kettle to remove impurity ions, polymers and conductive agent impurities.
In a preferred embodiment, the air pressure at the outlet of the Roots blower 4 is 10000h+ (1000-2000) Pa, wherein h is the height (unit is m) of the liquid level in the heating kettle.
NMP wastewater was purified using the above process under the specific conditions shown in tables 1 and 2:
TABLE 1
| Sequence number | Kettle liquid temperature （℃） | Roots blower fan Pressure (Pa) | Distillation 7- Internal pressure of the kettle of 10kPa Tower corresponding to force Top temperature (. Degree. C.) | Unit area integral Surface of sub-sieve membrane Impurity attachment amount （kg/m 2 ） | NMP product purity （wt，%） |
| 1 | 120 | 10000h+ （1000— 2000） | 118±1 | 0.01 | 99.8 |
| 2 | 120 | 10000h+ 10000 | 118±1 | 0.26 | 99.8 |
| 3 | 120 | 10000h+ （1000— 2000） | 126±1 | 0.01 | 99.7 |
| 4 | 120 | 10000h+ 10000 | 126±1 | 0.26 | 99.7 |
As can be seen from table 1, when the wind pressure of the Roots blower exceeds the set value, impurities adhere to the surface of the molecular sieve membrane group, thereby affecting the service life of the molecular sieve membrane group.
TABLE 2
| Sequence number | Process conditions | NMP content in permeate wastewater （wt，%） |
| 1 | If NMP waste liquid is directly fed in liquid phase Is put into a molecular sieve membrane group for circulation Ring, feeding temperature 120 ℃, condensation The temperature of the reactor is-15 to-10 DEG C Is a refrigerating fluid of (a); molecular sieve membrane group permeation Absolute pressure of the transmission side < 2kPa | 0.53 |
| 2 | The process of the invention | 0.02 |
| 3 | NMP waste liquid in heating kettle is 160 Other technological conditions and the present invention except at the temperature The same invention | 0.03 |
It can be seen from table 2 that if NMP waste liquid enters the molecular sieve membrane group in liquid phase instead of evaporated gas phase, the NMP content in the separated waste water is 0.53%, which is far higher than 0.02% of the present invention, and there is a higher requirement on the treatment capacity of the sewage station, and also has a negative effect on the NMP yield; in addition, the waste liquid directly contacts the molecular sieve membrane module in a liquid phase, wherein impurities can reduce the service life of the molecular sieve membrane module. When the temperature in the heating kettle is 160 ℃ and other process conditions are the same as those of the invention, the NMP content in the obtained osmotic wastewater is 0.03 percent, which is slightly higher than 0.02 percent of the process, and the treatment capacity of a sewage station is higher, and meanwhile, the energy consumption is increased and the cost is increased.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples only represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the claims. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
Claims (7)
1. An NMP waste liquid purification system, comprising: heating kettle, distillation tower, roots blower, buffer tank, molecular sieve membrane group, condenser, wastewater receiving tank, product receiving tank, vacuum buffer tank and vacuum pump;
the heating kettle is used for heating NMP waste liquid to be purified, the bottom of the heating kettle is provided with a gas distributor, and the gas outlet end at the top of the heating kettle is respectively connected with a distillation tower and a molecular sieve membrane group; the air inlet end of the gas distributor is connected with a Roots blower;
the distillation tower is used for separating the NMP waste liquid with qualified moisture, the air inlet end at the bottom of the distillation tower is connected with the air outlet end of the heating kettle, and the air outlet end at the top of the distillation tower is connected with the condenser;
the molecular sieve membrane group is used for separating NMP and water molecules in the circulating treatment gas; the inlet of the heating kettle is connected with the air outlet end of the heating kettle; the outlet of the upper end is connected with a condenser and discharges water molecules, and the outlet of the lower end is connected with a buffer tank and discharges NMP circulation treatment gas after removing a part of water molecules;
the Roots blower is used for circularly treating the air to be pressurized and then blown into the bottom of the heating kettle; the air inlet end of the air inlet pipe is connected with a buffer tank;
the condenser is used for condensing the distilled material steam, and the air inlet end of the condenser is connected with the air outlet end of the distillation tower and the upper end outlet of the molecular sieve membrane group; the air outlet end of the device is connected with a waste water receiving tank and a product receiving tank;
the vacuum buffer tank is used for reducing the pressure of the system, the inlet end of the vacuum buffer tank is respectively connected with the wastewater receiving tank and the product receiving tank, and the outlet end of the vacuum buffer tank is connected with the vacuum pump;
the vacuum pump is used for reducing pressure of the system and exhausting tail gas, and the inlet end of the vacuum pump is connected with the outlet end of the vacuum buffer tank.
2. An NMP waste liquid purification system according to claim 1, characterized in that said waste water receiving tank and product receiving tank are used for collecting waste water and NMP product, respectively.
3. The NMP waste liquid purification system of claim 1, wherein a valve is provided between said heating kettle and said distillation column.
4. A NMP waste liquid purification system according to claim 3, wherein a valve is provided between said heating kettle and molecular sieve membrane module.
5. The NMP waste liquid purification system of claim 1, wherein the molecular sieve in said molecular sieve membrane set is NaA molecular sieve with a pore size of 4A.
6. A process for purifying NMP waste liquid, characterized by being used in the system according to any one of claims 1 to 5, comprising the steps of:
adding NMP waste liquid to be purified into a heating kettle, removing non-condensable gas under the pressure of less than or equal to-0.099 MPa, closing a valve on the heating kettle, and heating to 120+/-5 ℃ until the temperature of the waste liquid is 120 ℃; when the Roots blower is started and the Roots blower blows air into the kettle liquid, the circulating treatment gas forms small bubbles which are uniformly distributed through the gas distributor, carries out heat and mass exchange with the kettle liquid, and water molecules enter the bubbles and then enter the gas phase of the liquid surface, and finally enter the molecular sieve membrane group to separate NMP and water molecules; at this time, the condenser is filled with a refrigerating fluid at the temperature of-15 to-10 ℃ and the absolute pressure of the permeation side of the molecular sieve membrane group is controlled to be less than 2kPa;
when the water content of NMP waste liquid circulated into the heating kettle is less than or equal to 100ppm, a valve of the heating kettle, which is communicated with a distillation tower, is opened, a valve communicated with a molecular sieve membrane group is closed, cooling water with the temperature less than or equal to 32 ℃ is introduced into a condenser, absolute pressure in the heating kettle is controlled to be 7-10kPa, kettle liquid temperature is controlled to be 128-134 ℃, distillation tower top temperature is controlled to be 118+/-1 ℃, and NMP in the kettle liquid is distilled out, so that impurity ions, polymers and conductive agent impurities are removed.
7. The process for purifying NMP waste liquid according to claim 6, wherein the air pressure at the outlet of the Roots blower is 10000h+ (1000-2000) Pa, wherein h is the height (m) of the liquid level in the heating kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310688422.1A CN116409839B (en) | 2023-06-12 | 2023-06-12 | NMP waste liquid purification system and technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310688422.1A CN116409839B (en) | 2023-06-12 | 2023-06-12 | NMP waste liquid purification system and technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116409839A true CN116409839A (en) | 2023-07-11 |
| CN116409839B CN116409839B (en) | 2023-08-08 |
Family
ID=87059726
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310688422.1A Active CN116409839B (en) | 2023-06-12 | 2023-06-12 | NMP waste liquid purification system and technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116409839B (en) |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090057128A1 (en) * | 2007-08-30 | 2009-03-05 | Leland Vane | Liquid separation by membrane assisted vapor stripping process |
| CN101973921A (en) * | 2010-09-29 | 2011-02-16 | 上海化学试剂研究所 | Method for removing methylamine and moisture in N-methyl pyrrolidone |
| KR20110050877A (en) * | 2009-11-09 | 2011-05-17 | 신상규 | Purification method of waste slurry from semiconductor and solar cell wafer manufacturing process and regenerating cutting fluid for semiconductor and solar cell wafer using them |
| CN107803319A (en) * | 2017-11-13 | 2018-03-16 | 林州朗坤科技有限公司 | A kind of NMP recovery purification systems and its recovery method of purification |
| CN109195688A (en) * | 2016-05-27 | 2019-01-11 | 三菱化学株式会社 | The dewatering system and its method of operation and dewatering of water-containing organic compound |
| JP2020146639A (en) * | 2019-03-14 | 2020-09-17 | オルガノ株式会社 | Dehydration apparatus and dehydration method of organic solvent |
| JP2020146635A (en) * | 2019-03-14 | 2020-09-17 | オルガノ株式会社 | Dehydrator and dehydration method for liquid mixture including organic solvent and water |
| CN211561936U (en) * | 2019-03-14 | 2020-09-25 | 奥加诺株式会社 | Organic solvent dehydration device and refining system |
| CN111892525A (en) * | 2020-05-08 | 2020-11-06 | 迈奇化学股份有限公司 | N-methyl pyrrolidone for liquid crystal panel and production process thereof |
| WO2021132869A1 (en) * | 2019-12-26 | 2021-07-01 | 주식회사 에너엔비텍 | Pervaporation membrane separation process for concentration of specific organic compound from wastewater containing the organic compound and wastewater treatment |
| CN215842408U (en) * | 2021-09-03 | 2022-02-18 | 深圳市德尼环保技术有限公司 | Lithium ion battery coating process NMP recovery unit |
| CN216725832U (en) * | 2021-11-24 | 2022-06-14 | 东莞市鹏锦机械科技有限公司 | High-efficient NMP waste liquid rectification purification device |
-
2023
- 2023-06-12 CN CN202310688422.1A patent/CN116409839B/en active Active
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090057128A1 (en) * | 2007-08-30 | 2009-03-05 | Leland Vane | Liquid separation by membrane assisted vapor stripping process |
| KR20110050877A (en) * | 2009-11-09 | 2011-05-17 | 신상규 | Purification method of waste slurry from semiconductor and solar cell wafer manufacturing process and regenerating cutting fluid for semiconductor and solar cell wafer using them |
| CN101973921A (en) * | 2010-09-29 | 2011-02-16 | 上海化学试剂研究所 | Method for removing methylamine and moisture in N-methyl pyrrolidone |
| CN109195688A (en) * | 2016-05-27 | 2019-01-11 | 三菱化学株式会社 | The dewatering system and its method of operation and dewatering of water-containing organic compound |
| CN107803319A (en) * | 2017-11-13 | 2018-03-16 | 林州朗坤科技有限公司 | A kind of NMP recovery purification systems and its recovery method of purification |
| JP2020146639A (en) * | 2019-03-14 | 2020-09-17 | オルガノ株式会社 | Dehydration apparatus and dehydration method of organic solvent |
| JP2020146635A (en) * | 2019-03-14 | 2020-09-17 | オルガノ株式会社 | Dehydrator and dehydration method for liquid mixture including organic solvent and water |
| CN211561936U (en) * | 2019-03-14 | 2020-09-25 | 奥加诺株式会社 | Organic solvent dehydration device and refining system |
| WO2021132869A1 (en) * | 2019-12-26 | 2021-07-01 | 주식회사 에너엔비텍 | Pervaporation membrane separation process for concentration of specific organic compound from wastewater containing the organic compound and wastewater treatment |
| CN111892525A (en) * | 2020-05-08 | 2020-11-06 | 迈奇化学股份有限公司 | N-methyl pyrrolidone for liquid crystal panel and production process thereof |
| CN215842408U (en) * | 2021-09-03 | 2022-02-18 | 深圳市德尼环保技术有限公司 | Lithium ion battery coating process NMP recovery unit |
| CN216725832U (en) * | 2021-11-24 | 2022-06-14 | 东莞市鹏锦机械科技有限公司 | High-efficient NMP waste liquid rectification purification device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116409839B (en) | 2023-08-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112933987B (en) | Organic solvent purification system and method | |
| JP6636111B2 (en) | Organic solvent purification system and method | |
| CN110938047B (en) | Tetrahydrofuran-benzene-water mixture separation process and device | |
| JP6415159B2 (en) | Organic solvent purification system and method | |
| CN105209153A (en) | Method for condensing water-soluble organic matter and device for condensing water-soluble organic matter | |
| CN113813623A (en) | MVR concentration and rectification system and recovery method of DMAC waste liquid | |
| CN116409839B (en) | NMP waste liquid purification system and technology | |
| CN111848348A (en) | Isopropyl alcohol dehydration refining method | |
| JP2020075865A (en) | Water-alcohol separation system and water-alcohol separation method for producing alcohol | |
| CN214004476U (en) | NMP device is refine in pervaporation membrane separation | |
| CN111909120B (en) | Energy-saving separation process of water-containing ternary azeotropic system | |
| CN215232207U (en) | Purification device of electronic-grade propionate | |
| US20220009864A1 (en) | A Separation Method and Reactor System for a Glycol-Water Mixture | |
| WO2019193951A1 (en) | Organic solvent purification system and method | |
| CN213060535U (en) | Permanent purple kneading wastewater treatment device | |
| CN214361095U (en) | Energy-saving separation device of water-containing ternary azeotropic system | |
| CN114452669B (en) | Reclaimed material liquid rectifying and purifying system containing NMP | |
| CN110468162B (en) | Production process and device for preparing fuel ethanol by one-time phase transition method | |
| CN212881891U (en) | Isopropanol pervaporation dehydration device | |
| CN219743939U (en) | Energy-saving tetrahydrofuran aqueous solution rectifying system | |
| CN111825639B (en) | Tetrahydrofuran dehydration refining method | |
| CN218944765U (en) | Zeolite membrane dewatering device for efficiently separating water in water-containing solvent | |
| CN217947874U (en) | DMAC waste water multiple-effect rectification device | |
| CN112439320A (en) | Method for separating and refining NMP (N-methyl pyrrolidone) by using pervaporation membrane | |
| CN117902654A (en) | Methanol and propylene glycol-containing wastewater treatment system and treatment method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |